Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of preparation method of 2-acetyl-2-desamidotetracycline

A technology of amidotetracycline and acetyl, which is applied in the field of biopharmaceuticals, can solve the problems of poor antibacterial activity and high toxicity, achieve the effect of simple process and solve the problem of impurity positioning

Active Publication Date: 2016-11-23
NINGXIA QIYUAN PHARMA
View PDF2 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation process of tetracycline hydrochloride will produce impurities, mainly including 4-epitetracycline (4-epitetracycline), 4-epianhydrotetracycline (4-epianhydrotetracycline), anhydrotetracycline (Anhydrotetracycline), oxytetracycline (Oxytetracycline) and 2- Acetyl-2-decarbamoyltetracycline (2-acetyl-2-decarbamoyltetracycline), these impurities are highly toxic and have poor antibacterial activity

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Chromatographic conditions: chromatographic column: Sinochrom ODS-AP 10um; mobile phase: 0.05% phosphoric acid solution-acetonitrile (85:15); flow rate: 24ml / min; detection wavelength: 254nm.

[0022] Instrument model: Dalian Elite P230 preparative liquid chromatograph.

[0023] Preparation:

[0024] The urea double salt mother liquor in the production process of tetracycline hydrochloride was concentrated under reduced pressure at 0.08MPa at 60°C to 1 / 4 of the original volume, and injected into a preparative high-performance liquid chromatograph to collect 2-acetyl-2-deamidotetracycline Solution during the peak period.

[0025] Adjust the separated 2-acetyl-2-deamidotetracycline solution to neutral with acetic acid, gradually add solid sodium chloride and stir until the acetonitrile and water layers are separated, separate the acetonitrile layer, and then add to the water layer Equal volume of acetonitrile, shake, stand still, separate the acetonitrile layer, combine...

Embodiment 2

[0027] Chromatographic conditions: chromatographic column: Sinochrom ODS-AP 10um; mobile phase: 0.05% phosphoric acid solution-acetonitrile (85:20); flow rate: 20ml / min; detection wavelength: 254nm.

[0028] Instrument model: Dalian Elite P230 preparative liquid chromatograph.

[0029] Preparation:

[0030] The urea double salt mother liquor in the production process of tetracycline hydrochloride was concentrated under reduced pressure at 0.06MPa at 58°C to 1 / 4 of its original volume, and injected into a preparative high-performance liquid chromatograph to collect 2-acetyl-2-deamidotetracycline Solution during the peak period.

[0031] Adjust the separated 2-acetyl-2-deamidotetracycline solution to neutral with acetic acid, gradually add solid sodium chloride and stir until the acetonitrile and water layers are separated, separate the acetonitrile layer, and then add to the water layer Equal volume of acetonitrile, shake, stand still, separate the acetonitrile layer, combine...

Embodiment 3

[0033] Chromatographic conditions: chromatographic column: Sinochrom ODS-AP 10um; mobile phase: 0.05% phosphoric acid solution-acetonitrile (85:20); flow rate: 20ml / min; detection wavelength: 254nm.

[0034] Instrument model: Dalian Elite P230 preparative liquid chromatograph.

[0035] Preparation:

[0036] The urea double salt mother liquor in the production process of tetracycline hydrochloride was concentrated under reduced pressure at 0.09MPa at 62°C to 1 / 4 of the original volume, and injected into a preparative high-performance liquid chromatograph to collect 2-acetyl-2-deamidotetracycline Solution during the peak period.

[0037] Adjust the separated 2-acetyl-2-deamidotetracycline solution to neutral with acetic acid, gradually add solid sodium chloride and stir until the acetonitrile and water layers are separated, separate the acetonitrile layer, and then add to the water layer Equal volume of acetonitrile, shake, stand still, separate the acetonitrile layer, combine...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
wavelengthaaaaaaaaaa
Login to View More

Abstract

The present invention relates to a 2-acetyl-2-desamino methyl tetracycline preparation method. According to the method, an urea double salt mother liquor during a tetracycline hydrochloride production process is subjected to pressure reducing concentrating and then is injected into a high performance liquid chromatograph, a 2-acetyl-2-desaminomethyl tetracycline solution is collected, the pH value of the separated 2-acetyl-2-desaminomethyl tetracycline solution is adjusted to a neutral pH value, sodium chloride is added gradually so as to achieve layering of acetonitrile and water, the 2-acetyl-2-desaminomethyl tetracycline is extracted into the acetonitrile layer, separation is performed to take the acetonitrile layer, an appropriate amount of acetonitrile is added to the water layer, shaking and standing are sequentially performed, separation is performed to take the acetonitrile layer, the acetonitrile layers obtained from the two separations are mixed, the obtained acetonitrile is placed into a freezing chamber of a refrigerator to stand overnight and then is taken out and immediately filtered, the filtrate is taken, and is sequentially subjected to pressure reducing concentrating and drying to obtain the 2-acetyl-2-desamino methyl tetracycline pure product. The preparation method of the present invention has characteristics of simple process, efficiency, rapidness, high recovery rate and the like.

Description

technical field [0001] The invention belongs to the technical field of biopharmaceuticals, in particular to a preparation method of 2-acetyl-2-desamidotetracycline. Background technique [0002] Tetracycline hydrochloride is a tetracyclic antibiotic, which has a good inhibitory effect on Gram-positive bacteria, negative bacteria, rickettsia, viral viruses, spirochetes and protozoa. Tetracycline hydrochloride is fermented by Streptococcus aureus at 32°C for 170 hours, the fermented liquid is acidified at pH 1.7-1.9, filtered, the filtrate is adjusted to pH and crystallized to obtain tetracycline, tetracycline and urea react to form tetracycline urea double salt, tetracycline urea double salt After adding hydrochloric acid to alcohol, the reaction produces tetracycline hydrochloride. The preparation process of tetracycline hydrochloride will produce impurities, mainly including 4-epitetracycline (4-epitetracycline), 4-epianhydrotetracycline (4-epianhydrotetracycline), anhydro...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07C237/26C07C231/24
Inventor 周红邹学锋李鑫
Owner NINGXIA QIYUAN PHARMA